Hydrochloric Acid → N-[1-(5,5,8,8-tetramethyl-6,7-dihydronaphthalen-2-yl)ethylidene]hydroxylamine

HRID 2259806노트

반응식

HRID 2259806 반응식
[C:1]([C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][CH:13]=1)[C:10]([CH3:15])([CH3:14])[CH2:9][CH2:8][C:7]2([CH3:17])[CH3:16])(=O)[CH3:2].[Cl-].[OH:19][NH3+:20].Cl>N1C=CC=CC=1>[N:20](=[C:1]([C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][CH:13]=1)[C:10]([CH3:15])([CH3:14])[CH2:9][CH2:8][C:7]2([CH3:17])[CH3:16])[CH3:2])[OH:19]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 21645Hydroxylamine HClHCID 27475621-(5,5,8,8-Tetramethyl-5,6,7,8-tetrahydronaphthalen-2-yl)ethan-1-one

생성물 1

HCID 2747574N-[1-(5,5,8,8-tetramethyl-6,7-dihydronaphthalen-2-yl)ethylidene]hydroxylamine수율 100.3%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

15 g (65 millimoles) of 6-acetyl-1,2,3,4-tetrahydro-1,1,4,4-tetramethylnaphthalene and 6.5 g (91 millimoles) of hydroxylammonium chloride in 100 ml of pyridine were heated for 1 hour at 80° C. After cooling, the mixture was poured onto water and acidified with 2N hydrochloric acid. The precipitated crystals were filtered off under suction, washed with water and dried. 16 g of 6-[1-hydroximinoethyl]-1,2,3,4-tetrahydro-1,1,4,4-tetramethylnaphthalene were obtained in this manner. 5 g (20 millimoles) thereof and 5 g (20 millimoles) of terephthalic monomethyl ester chloride were combined and were stirred for 6 hours at 120° C. After cooling, the solidified material was dissolved with about 60 ml of methanol. The supernatant methanol phase was decanted and the solid residue was recrystallized twice from chloroform/methanol. 2.5 g of the title compound of melting point 207°-208° C. were obtained in this manner.

후처리

  1. temperatureAfter cooling
  2. additionthe mixture was poured onto water
  3. filtrationThe precipitated crystals were filtered off under suction
  4. washwashed with water
  5. customdried

출처 및 근거

ORD 기록
ord-8715286588d746018b72e43fee575fcd
출처 데이터셋
uspto-grants-1995_12
특허 번호
US05475017

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